CN114832638A - Method and device for post-treating polymer membrane by utilizing sodium hypochlorite to regulate and control pore size of polymer membrane - Google Patents
Method and device for post-treating polymer membrane by utilizing sodium hypochlorite to regulate and control pore size of polymer membrane Download PDFInfo
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- CN114832638A CN114832638A CN202210527798.XA CN202210527798A CN114832638A CN 114832638 A CN114832638 A CN 114832638A CN 202210527798 A CN202210527798 A CN 202210527798A CN 114832638 A CN114832638 A CN 114832638A
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- 239000005708 Sodium hypochlorite Substances 0.000 title claims abstract description 87
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000011148 porous material Substances 0.000 title claims abstract description 19
- 229920005597 polymer membrane Polymers 0.000 title claims description 26
- 239000012528 membrane Substances 0.000 claims abstract description 76
- 229920006254 polymer film Polymers 0.000 claims abstract description 25
- 229920002492 poly(sulfone) Polymers 0.000 claims description 40
- 238000003860 storage Methods 0.000 claims description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 14
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008213 purified water Substances 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000008280 blood Substances 0.000 description 7
- 210000004369 blood Anatomy 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000001631 haemodialysis Methods 0.000 description 1
- 230000000322 hemodialysis Effects 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000009285 membrane fouling Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The invention provides a method for post-treating a polymer film by utilizing sodium hypochlorite to regulate and control the aperture size of the polymer film, which adopts sodium hypochlorite solution to post-treat the polymer film. The invention provides a method for directly using a sodium hypochlorite solution to treat a PS/PVP membrane to regulate and control the pore size of the PS/PVP membrane.
Description
Technical Field
The invention relates to the technical field, in particular to a method and a device for regulating and controlling the aperture size of a polymer film by post-treating the polymer film with sodium hypochlorite.
Background
Polysulfone (PS) has many excellent properties such as chemical inertness over the entire pH range, compressive strength, thermal stability (150-170 ℃) and mechanical strength (fracture, bending, torsion) and is therefore one of the most popular synthetic polymeric materials for the manufacture of membranes. In recent years, hydrophilic PS/PVP membranes modified by hydrophilic additives such as polyvinylpyrrolidone (PVP) have been widely used in the fields of microfiltration/ultrafiltration, hemodialysis, plasma separator, membrane oxygenator, cell culture, bioartificial organs, and the like.
A key factor in the development and application of polymer films is the control of their polymer morphology. The membrane pore size and porosity are controlling factors of the membrane morphology, which can improve membrane performance and reduce membrane fouling. The regulation range of the surface aperture of the PS/PVP membrane synthesized by PVP as a pore-foaming agent and a surface modifier is smaller. Post-processing is one of the processing ways to control the film morphology to improve the performance of the PS film.
The existing method for regulating and controlling the aperture size of the PS/PVP membrane yarn mainly comprises heat treatment and plasma treatment. The heat treatment is a post-treatment by heating the PS film to 185 ℃, the temperature is increased to 185 ℃, the fiber diameter begins to decrease significantly, and the decrease in fiber diameter results in an increase in the porosity of the film. The method needs higher temperature and has smaller change range of the membrane aperture size.
In plasma processing, the plasma acts on the PS film similarly to oxidative etching, making the pores larger and the size distribution wider. The membrane with the required pore diameter can be obtained by adopting a plasma modification method. A piece of the film was placed in the plasma reactor, the apparatus was opened, and the desired film was obtained within a few seconds. Furthermore, the amount of waste generated is rather limited (modification in the gas phase). However, the method needs more complex equipment, has higher investment cost, and is difficult to control the post-treatment of the hollow fiber membrane. It is therefore desirable to find a more convenient method of membrane post-treatment.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method and a device for controlling the pore size of a polymer membrane by post-treating the polymer membrane with sodium hypochlorite, wherein the mechanical properties of the polymer membrane are not affected while the pore size of the polymer membrane is controlled, and the operation is convenient.
The invention provides a method for post-treating a polymer film by utilizing sodium hypochlorite to regulate the aperture size of the polymer film, and the polymer film is post-treated by adopting a sodium hypochlorite solution.
The regulation and control of the invention means that the enlargement of the polymer film hole is realized, and particularly, the controllability of the enlargement of the polymer film hole is realized through different temperatures, times and concentrations of sodium hypochlorite treatment.
Preferably, the sodium hypochlorite solution is a sodium hypochlorite aqueous solution, wherein the concentration of sodium hypochlorite is 50 to 5000ppm, more preferably 250 to 2000ppm, and in some embodiments of the invention, the concentration of sodium hypochlorite is 50, 100, 150, 200, 250, 300, 350, 400, 450, 500, 1000, 1500, 2000, 2500, 3000, 3500, 4000, 4500 or 5000ppm, or any of the above values is an upper limit or a lower limit.
In the invention, the pH value of the sodium hypochlorite solution is preferably more than or equal to 9.5, and more preferably 11-11.5.
In the present invention, the polymer membrane may be a polysulfone/polyvinylpyrrolidone (PS/PVP) membrane, and may be used for water treatment, dialysate filters, hemodialyzers, and the like.
Preferably, the temperature of the post-treatment is not higher than 40 ℃, more preferably 25 to 40 ℃, and in some embodiments, the temperature of the post-treatment is 25, 30, 35 or 40 ℃, or any of the above values is a range of upper or lower limits.
In the invention, the time of the post-treatment is preferably 0.1-50 h, and more preferably 1-5 h.
The flow chart of the above-mentioned post-treatment of the polymer film with sodium hypochlorite is shown in FIG. 1.
In another aspect, the present invention provides a device for post-treating a polymer membrane with sodium hypochlorite to control the pore size thereof, comprising:
the device comprises a sodium hypochlorite solution storage device, a polysulfone membrane component, a first pipeline, a second pipeline and/or a third pipeline;
one end of the first pipeline is connected with the sodium hypochlorite solution storage device, the other end of the first pipeline is connected with the inside of the polymer membrane through the bottom end of the polysulfone membrane component, and the first pipeline is provided with a pump;
one end of the second pipeline is connected with the sodium hypochlorite solution storage device, and the other end of the second pipeline is connected with the inside of the polymer membrane through the top end of the polysulfone membrane component;
one end of the third pipeline is connected with the sodium hypochlorite solution storage device, and the other end of the third pipeline is connected with the outside of the polymer membrane through the side wall of the polysulfone membrane component.
The schematic of the above-described device is shown in fig. 2.
Wherein, sodium hypochlorite solution strorage device is used for holding sodium hypochlorite solution.
The polysulfone membrane component is used for containing the membrane thread component.
The first pipeline is used for introducing a sodium hypochlorite solution into the membrane filament assembly membrane.
The membrane of the present invention refers to the hollow bore section inside the membrane filaments, i.e. the blood compartment. Extramembranous refers to the outside of the membrane filament, i.e., the dialysate compartment.
The second pipeline is used for enabling the sodium hypochlorite solution to pass through the membrane and return to the sodium hypochlorite solution storage device from the top end of the polysulfone membrane module.
When the system opens the first pipeline and the second pipeline, the polysulfone membrane module is treated in the membrane, and sodium hypochlorite solution flows in from one end of the aperture of the membrane module and flows out from the other end of the aperture of the membrane module.
The third pipeline is used for enabling the sodium hypochlorite solution to move from the inside of the membrane to the outside of the membrane under the driving of pressure, and returning the sodium hypochlorite solution to the sodium hypochlorite solution storage device from the side wall of the polysulfone membrane module.
When the system opens the first pipeline and the third pipeline, the polysulfone membrane module is treated from the inside to the outside of the membrane, sodium hypochlorite solution flows into the membrane from one end of the membrane module, moves to the outside of the membrane through the membrane under the driving of pressure, and returns to the sodium hypochlorite solution storage device through the third pipeline.
When setting up first pipeline, second pipeline and third pipeline simultaneously, can set up the stagnant water clamp on the pipeline, the flow direction of control sodium hypochlorite solution. The first pipeline, the second pipeline and the third pipeline can be opened simultaneously, and the membrane inside mode and the membrane inside and outside mode are carried out simultaneously.
In another aspect, the present invention provides a method for post-treating a polymer film using the above apparatus, comprising the steps of:
s1) installing a polymer membrane in the polysulfone membrane module, and opening the first and third lines;
s2) pumping the sodium hypochlorite solution into the membrane through a first pipeline, driving the sodium hypochlorite solution to move outside the membrane through the membrane under the drive of pressure, and returning the sodium hypochlorite solution to a sodium hypochlorite solution storage device through a third pipeline;
s3), the polymer film was rinsed with purified water until no sodium hypochlorite remained.
Specifically, firstly, a certain amount of 5% -10% sodium hypochlorite concentrated solution is measured, diluted to the concentration of 50-5000 ppm in proportion, HCl/NaOH is used for adjusting the pH value of the solution to be not less than 9.5, and the solution is placed in a sodium hypochlorite solution storage device.
In some embodiments of the present invention, the sodium hypochlorite solution storage device may be a container such as a general storage tank, and the present invention is not limited thereto.
And then the polymer membrane is arranged in the polysulfone membrane component, sodium hypochlorite solution is pumped into the membrane through the first pipeline, and the post-treatment of the polymer membrane is realized by controlling the switches of the second pipeline and the third pipeline.
During the pumping process, the pumping speed is preferably 300-1000 mL/min, and in some embodiments of the present invention, the pumping speed is 300, 400, 500, 600, 700, 800, 900 or 1000mL/min, or any of the above values is an upper or lower range.
Preferably, in the present invention, the step S3) is specifically:
and circulating for 0.1-50 h at the temperature of less than or equal to 40 ℃, and washing the polymer film with purified water until no sodium hypochlorite remains.
Compared with the prior art, the invention provides a method for post-treating the polymer film by utilizing sodium hypochlorite to regulate and control the aperture size of the polymer film, and the sodium hypochlorite solution is used for post-treating the polymer film.
The invention provides a method for directly using a sodium hypochlorite solution to treat a PS/PVP membrane to regulate and control the pore size of the PS/PVP membrane.
Drawings
FIG. 1 is a flow diagram of the present invention for post-treatment of a polymer film with sodium hypochlorite;
fig. 2 is a schematic structural diagram of the device for post-treating a polymer membrane with sodium hypochlorite to control the pore size of the polymer membrane provided by the invention.
Detailed Description
In order to further illustrate the present invention, the following examples are provided to describe the method and apparatus for controlling the pore size of the polymer membrane by post-treating the polymer membrane with sodium hypochlorite.
Example 1
2L sodium hypochlorite solutions (pH 10, 10.5, 11, 11.5) were prepared at 250, 500, 1000, 2000ppm, respectively. The pipeline and the polysulfone membrane component are connected according to the experimental device shown in FIG. 2, and the first pipeline and the second pipeline are opened for pre-charging and exhausting. And pumping the sodium hypochlorite solution into a blood chamber of the polysulfone membrane component at a pump speed of 700mL/min, closing the second pipeline, driving the sodium hypochlorite solution to move across the membrane under the driving of pressure to enter a dialysate chamber, opening the third pipeline, and returning the sodium hypochlorite solution to the sodium hypochlorite solution storage device through the third pipeline. After 1 hour of circulation at 25 ℃, the blood and dialysate compartments were rinsed with purified water until no sodium hypochlorite remained. The membrane pore size test was performed and the results are shown in table 1.
TABLE 1 average pore diameter of PS/PVP membrane after sodium hypochlorite treatment at different concentrations
Example 2
29mL of a 5% sodium hypochlorite solution was dissolved in 1421mL of purified water to give a 1000ppm aqueous sodium hypochlorite solution, which was adjusted to pH 11.5 with NaOH. The pipeline and the polysulfone membrane component are connected according to the experimental device shown in FIG. 2, and the first pipeline and the second pipeline are opened for pre-charging and exhausting. Pumping 1000ppm sodium hypochlorite solution into a blood chamber of the polysulfone membrane component at the pump speed of 700mL/min, alternately opening the second pipeline and the third pipeline to enable the sodium hypochlorite solution to alternately circulate inside and outside the membrane of the polysulfone membrane component, circulating at 40 ℃ for 5 hours, and then washing the blood chamber and the dialysate chamber with purified water until no sodium hypochlorite remains. The membrane pore size test was performed and the results are shown in table 2.
TABLE 240 ℃ average pore diameter of PS/PVP membrane before and after 1000ppm sodium hypochlorite treatment for 5 hours
Example 3
29mL of 5% sodium hypochlorite solution was dissolved in 1421mL of purified water to obtain 1000ppm of sodium hypochlorite aqueous solution, and the pH of the solution was adjusted to 8 and 11 with HCl and NaOH, respectively. The pipeline and the polysulfone membrane component are connected according to the experimental device shown in FIG. 2, and the first pipeline and the second pipeline are opened for pre-charging and exhausting. And pumping 1000ppm sodium hypochlorite solution into a blood chamber of the polysulfone membrane component at a pump speed of 700mL/min, closing the second pipeline, enabling the sodium hypochlorite solution to move across the membrane under the driving of pressure to enter a dialysate chamber, opening the third pipeline, and returning to the sodium hypochlorite solution storage device through the third pipeline. After 1 hour of circulation at 25 ℃, the blood and dialysate compartments were rinsed with purified water until no sodium hypochlorite remained. The tensile strength test of the film was carried out, and the results are shown in Table 3.
TABLE 3 tensile Strength of PS/PVP films before and after treatment with different pH and 1000ppm sodium hypochlorite
| pH of treatment liquid | Untreated | 8 | 11 |
| Tensile strength (MPa) | 6.422 | 5.814 | 6.409 |
The above examples show that the polysulfone membrane is treated by sodium hypochlorite, and the pore diameter of the membrane can be well regulated and controlled by adjusting parameters.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A method for post-treating a polymer film by utilizing sodium hypochlorite to regulate the pore size of the polymer film adopts sodium hypochlorite solution to post-treat the polymer film.
2. The method according to claim 1, wherein the sodium hypochlorite solution is an aqueous sodium hypochlorite solution, wherein the concentration of the sodium hypochlorite is 50-5000 ppm.
3. The method of claim 1, wherein the pH of the sodium hypochlorite solution is 9.5 or greater.
4. The method of claim 1, wherein the polymer membrane is a polysulfone/polyvinylpyrrolidone membrane.
5. The method according to claim 1, characterized in that the temperature of the post-treatment is less than or equal to 40 ℃.
6. The method according to claim 1, wherein the post-treatment time is 0.1 to 50 hours.
7. An apparatus for post-treating a polymer membrane with sodium hypochlorite to control its pore size, comprising:
the device comprises a sodium hypochlorite solution storage device, a polysulfone membrane component, a first pipeline, a second pipeline and/or a third pipeline;
one end of the first pipeline is connected with the sodium hypochlorite solution storage device, the other end of the first pipeline is connected with the inside of the polymer membrane through the bottom end of the polysulfone membrane component, and the first pipeline is provided with a pump;
one end of the second pipeline is connected with the sodium hypochlorite solution storage device, and the other end of the second pipeline is connected with the inside of the polymer membrane through the top end of the polysulfone membrane component;
one end of the third pipeline is connected with the sodium hypochlorite solution storage device, and the other end of the third pipeline is connected with the outside of the polymer membrane through the side wall of the polysulfone membrane component.
8. A method of post-treating a polymer film using the apparatus of claim 7, comprising the steps of:
s1) installing a polymer membrane in the polysulfone membrane module, and opening the first and third lines;
s2) pumping the sodium hypochlorite solution into the membrane through a first pipeline, driving the sodium hypochlorite solution to move outside the membrane through the membrane under the drive of pressure, and returning the sodium hypochlorite solution to a sodium hypochlorite solution storage device through a third pipeline;
s3), the polymer film was rinsed with purified water until no sodium hypochlorite remained.
9. The method according to claim 8, wherein the step S3) is specifically:
and circulating for 0.1-50 h at the temperature of less than or equal to 40 ℃, and washing the polymer film with purified water until no sodium hypochlorite remains.
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